Lelli, M., et al., Solid-State Dynamic Nuclear Polarization at 9.4 and 18.8 T from 100 K to Room Temperature. J Am Chem Soc, 2015. 137(46): p. 14558-61.
Efficient dynamic nuclear polarization (DNP) in solids, which enables very high sensitivity NMR experiments, is currently limited to temperatures of around 100 K and below. Here we show how by choosing an adequate solvent, (1)H cross effect DNP enhancements of over 80 can be obtained at 240 K. To achieve this we use the biradical TEKPol dissolved in a glassy phase of ortho-terphenyl (OTP). We study the solvent DNP enhancement of both TEKPol and BDPA in OTP in the range from 100 to 300 K at 9.4 and 18.8 T. Surprisingly, we find that the DNP enhancement decreases only relatively slowly for temperatures below the glass transition of OTP (Tg = 243 K), and (1)H enhancements around 15-20 at ambient temperature can be observed. We use this to monitor molecular dynamic transitions in the pharmaceutically relevant solids Ambroxol and Ibuprofen.
Is solid-state NMR enhanced by dynamic nuclear polarization?
From The DNP-NMR Blog:
Is solid-state NMR enhanced by dynamic nuclear polarization?
Lee, D., S. Hediger, and G. De Paepe, Is solid-state NMR enhanced by dynamic nuclear polarization? Solid State Nucl Magn Reson, 2015. 66-67C(0): p. 6-20.
http://www.ncbi.nlm.nih.gov/pubmed/25779337
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05-02-2015 02:38 AM
Synthesis and evaluation of nitroxide-based oligoradicals for low-temperature dynamic nuclear polarization in solid state NMR
From The DNP-NMR Blog:
Synthesis and evaluation of nitroxide-based oligoradicals for low-temperature dynamic nuclear polarization in solid state NMR
Yau, W.-M., K.R. Thurber, and R. Tycko, Synthesis and evaluation of nitroxide-based oligoradicals for low-temperature dynamic nuclear polarization in solid state NMR. J. Magn. Reson., 2014(0).
http://www.sciencedirect.com/science/article/pii/S1090780714001372
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05-28-2014 04:28 PM
Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control
From The DNP-NMR Blog:
Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control
Sakaguchi, S., et al., Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, 2013. 317(0): p. 679-684.
http://www.sciencedirect.com/science/article/pii/S0168583X13008872
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01-23-2014 01:37 AM
Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control
From The DNP-NMR Blog:
Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control
Sakaguchi, S., et al., Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, 2013(0).
http://www.sciencedirect.com/science/article/pii/S0168583X13008872
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11-21-2013 01:14 AM
Dynamic Nuclear Polarization Enhanced NMR in the Solid-State
From The DNP-NMR Blog:
Dynamic Nuclear Polarization Enhanced NMR in the Solid-State
Akbey, Ü., et al., Dynamic Nuclear Polarization Enhanced NMR in the Solid-State. 2013, Springer Berlin Heidelberg. p. 1-48.
http://dx.doi.org/10.1007/128_2013_436
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08-26-2013 08:46 PM
[NMR paper] Dynamic Nuclear Polarization Enhanced NMR in the Solid-State.
Dynamic Nuclear Polarization Enhanced NMR in the Solid-State.
Dynamic Nuclear Polarization Enhanced NMR in the Solid-State.
Top Curr Chem. 2013 Jul 7;
Authors: Akbey U, Franks WT, Linden A, Rydmark MO, Lange S, Oschkinat H
Abstract
Nuclear magnetic resonance (NMR) spectroscopy is one of the most commonly used spectroscopic techniques to obtain information on the structure and dynamics of biological and chemical materials. A variety of samples can be studied including solutions, crystalline solids, powders and hydrated protein...
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07-09-2013 02:47 PM
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K
January 2013
Publication year: 2013
Source:Journal of Magnetic Resonance, Volume 226</br>
</br>
We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20–25K and 9.4Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier , but also includes a corrugated waveguide for transmission of microwaves from...
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12-15-2012 09:51 AM
Dynamic nuclear polarization experiments at 14.1 T for solid-state NMR.
Dynamic nuclear polarization experiments at 14.1 T for solid-state NMR.
Related Articles Dynamic nuclear polarization experiments at 14.1 T for solid-state NMR.
Phys Chem Chem Phys. 2010 Jun 14;12(22):5799-803
Authors: Matsuki Y, Takahashi H, Ueda K, Idehara T, Ogawa I, Toda M, Akutsu H, Fujiwara T
Instrumentation for high-field dynamic nuclear polarization (DNP) at 14.1 T was developed to enhance the nuclear polarization for NMR of solids. The gyrotron generated 394.5 GHz submillimeter (sub-mm) wave with a power of 40 W in the second harmonic...
Solid-State Dynamic Nuclear Polarization at 9.4 and 18.8 T from 100 K to Room Temperature
Linear Mode
